CN113861622A - Preparation of buoyancy material by integral forming process - Google Patents
Preparation of buoyancy material by integral forming process Download PDFInfo
- Publication number
- CN113861622A CN113861622A CN202111193591.5A CN202111193591A CN113861622A CN 113861622 A CN113861622 A CN 113861622A CN 202111193591 A CN202111193591 A CN 202111193591A CN 113861622 A CN113861622 A CN 113861622A
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- Prior art keywords
- filling
- preparation
- curing agent
- hollow glass
- curing
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C37/00—Component parts, details, accessories or auxiliary operations, not covered by group B29C33/00 or B29C35/00
- B29C37/0078—Measures or configurations for obtaining anchoring effects in the contact areas between layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/58—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres
- B29C70/66—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres the filler comprising hollow constituents, e.g. syntactic foam
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention relates to preparation of a buoyancy material by an integral forming process, in particular to a preparation method of a light integrated composite material. One of the purposes of the invention is to solve the problem of large heat release in the curing process of the large-volume buoyancy material under the normal-temperature curing condition, and provide a preparation process for filling the mold step by step for many times. The invention adopts a step-by-step multiple filling process, the filling amount of one time is controlled within a certain thickness, the heat emitted by the product in the curing process can be diffused in time, and the quality of the product cannot be reduced. The second purpose of the invention is to solve the problem that the process of the large-size floating body with simple size is complex, and provide a one-step forming preparation process. The floating body is basically formed by bonding and processing the standard module of the buoyancy material, and the preparation process provided by the invention omits a bonding processing procedure, simplifies the preparation process and improves the production efficiency of products.
Description
Technical Field
The invention relates to the field of light pressure-resistant composite materials, and mainly relates to a pressure-resistant composite material for shallow sea.
Background
The floating body for the marine device is mainly prepared by filling epoxy resin with hollow glass beads through a certain preparation process. Since the 21 st century, exploration and exploitation of marine mineral resources, marine environment monitoring and the like are increased in various countries in the world. The solid buoyancy material is used as an important matching material of deep sea equipment, and mainly provides buoyancy for the deep sea equipment and provides certain strength for the deep sea equipment. At present, most of floating bodies are formed into floating bodies with specific shapes mainly through standard modules of buoyancy materials after a bonding processing procedure. The invention mainly aims at the floating bodies with regular shapes and larger volumes or more quantities, and the floating bodies which can be directly used without processing or simple milling treatment are prepared by step-by-step and multiple filling.
Disclosure of Invention
One of the purposes of the invention is to solve the problem of large heat release in the curing process of the large-volume buoyancy material under the normal-temperature curing condition, and provide a preparation process for filling the mold step by step for many times. The invention adopts a step-by-step multiple filling process, the filling amount of one time is controlled within a certain thickness, the heat emitted by the product in the curing process can be diffused in time, and the quality of the product cannot be reduced.
The second purpose of the invention is to solve the problem that the process of the large-size floating body with simple size is complex, and provide a one-step forming preparation process. The floating body is basically formed by bonding and processing the standard module of the buoyancy material, and the preparation process provided by the invention omits a bonding processing procedure, simplifies the preparation process and improves the production efficiency of products.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the light integrated composite material is prepared by uniformly mixing the resin curing agent light filler and the like, filling the mixture into a mold with a certain shape for many times, and curing at room temperature or medium temperature to obtain a finished product.
In the above technical scheme, the resin is at least one of bisphenol a type epoxy resin, bisphenol F type epoxy resin, and unsaturated polyester resin.
In the above technical solution, the curing agent is a curing agent for thermosetting resin, and preferably at least one of a polyamide curing agent, a T31 curing agent, and isophorone diamine.
The light filler is hollow glass beads, and the density of the light filler is 0.125-0.42 g/cm3The hollow glass beads are treated by titanate or silane coupling agents before use.
In the technical scheme, the solid buoyancy material prepared by filling adopts the following raw materials in proportion:
in the above technical scheme, the preparation method comprises the following steps:
(1) the hollow glass beads are treated by adopting a coupling agent, the coupling agent and absolute ethyl alcohol are uniformly mixed, the mass fraction of the coupling agent is 10-20 wt%, then the selected hollow glass beads are added into a coupling agent ethanol solution according to the proportion of 1 wt%, and after a series of operations such as reflux washing, suction filtration, washing and drying, the modified hollow glass beads are obtained.
(2) Adding the weighed resin, curing agent, diluent and the like into a vacuum stirrer, controlling the stirring time to be 5-20 min according to the viscosity of the mixed solution, adding the weighed modified hollow glass microspheres after the mixed solution is uniformly stirred and defoamed, and continuing to stir in vacuum for 10-30 min.
(3) And filling the mixed and vacuum-treated material into a mold, controlling the filling thickness to be preferably 1-8 cm, keeping the material flat as much as possible, and curing the material at room temperature or medium-low temperature for 2-6 hours.
(4) And a layer of resin curing agent gel is coated on the filling material, so that the binding force between the filled material and the material to be filled is increased. And (4) repeating the steps (1) to (3) when the glue is not completely cured until the mould is filled.
(5) In the last filling procedure, the filling material is higher than the mould by about 1mm, and the filling material is machined into a regular size after being solidified; or a female die is added in the last filling procedure to control the shape and the size of the material.
In the technical scheme, the curing temperature in the step (3) is controlled to be 0-50 ℃.
Compared with the prior art, the invention has the following beneficial effects: the invention adopts a step-by-step filling mode, on one hand, the size of the mould is not limited, on the other hand, the curing degree of the filled buoyancy material is uniform, and the performance is consistent.
Detailed Description
The present invention is described in detail below with reference to specific examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art should make some insubstantial modifications and adaptations of the present invention based on the present disclosure.
The various raw materials and auxiliary agents used in the embodiments of the present invention are commercially available.
The raw material components are calculated according to the mass portion.
Example 1
Preparing a semi-cylindrical buoyancy material:
(1) VS5500 hollow glass microspheres were treated with KH-560 coupling agent. Uniformly mixing a coupling agent and absolute ethyl alcohol, wherein the mass fraction of the coupling agent is 10-20 wt%, then adding the selected hollow glass beads into a coupling agent ethanol solution according to the proportion of 1 wt%, and carrying out a series of operations such as refluxing, washing, suction filtering, washing, drying and the like to obtain the modified hollow glass beads.
(2) Weighing the E-51 resin, the polyamide 300# curing agent and the JX-017 diluent according to the mass ratio of 100: :70: 2, stirring the mixture in a vacuum stirrer at normal temperature for 5min in vacuum, adding the weighed modified hollow glass microspheres (180 parts) after the mixed solution is stirred uniformly and bubbles are removed, and continuing stirring the mixture in vacuum for 10min at normal temperature.
(3) And filling the mixed and vacuum-treated material into a mold, controlling the filling thickness to be 5cm, keeping the material flat as much as possible, and curing the material at room temperature for 4 hours.
(4) A thin layer of resin curing agent clear gel (E-51 resin and polyamide 300# curing agent in a ratio of 100:70) is coated on the filling material to increase the bonding force between the filled material and the material to be filled. And (4) repeating the steps (1) to (3) when the glue is not completely cured until the mould is filled.
(5) And in the last filling process, the filling material is 1mm higher than the mold, a female mold is added on the upper surface, an F clamp or a vulcanizing machine is used for pressurizing, and demolding is carried out after solidification is finished to obtain a corresponding buoyancy material product.
The semi-cylindrical buoyancy material prepared in the embodiment is obtained by weighing the weight of the buoyancy material by using an electronic scale, measuring the size of the buoyancy material by using a caliper and a tape measure to obtain the corresponding volume, and calculating to obtain the density of 0.46g/cm3And the water absorption rate is 0.2 percent under the hydrostatic pressure of 20MPa for 6 hours.
Example 2
Preparation of hemispherical float (diameter 60cm)
The example 2 is basically consistent with the example 1 in raw materials and process, and the difference is that: (1) the hemispherical floating body is filled in two steps. (2) The adopted hollow glass bead is HGS8000X, and the mass part of the hollow glass bead relative to the epoxy resin is 150 parts.
The hemispherical floating body prepared in this example was weighed using an electronic scale, and the dimensions of the buoyant material were measured using a caliper and a tape measure to obtain the corresponding volume, which was calculated to obtain a density of 0.53g/cm3And the water absorption rate is 0.42 percent under the hydrostatic pressure of 30MPa for 6 hours.
Claims (7)
1. The preparation method of the light integrated composite material is characterized by comprising the following steps of:
(1) treating hollow glass beads with a coupling agent, uniformly mixing the coupling agent with absolute ethyl alcohol, wherein the mass fraction of the coupling agent is 10-20 wt%, then adding the selected hollow glass beads into an ethanol solution of the coupling agent according to the proportion of 1 wt%, and performing a series of operations such as refluxing, washing, suction filtration, washing, drying and the like to obtain modified hollow glass beads;
(2) adding the weighed resin, curing agent, diluent and the like into a vacuum mixer, controlling the mixing time to be 5-20 min according to the viscosity of the mixed solution, adding the weighed modified hollow glass microspheres after the mixed solution is uniformly mixed and defoamed, and continuing to stir in vacuum for 10-30 min;
(3) filling the mixed and vacuum-treated material into a mold, controlling the filling thickness to be 1-8 cm, keeping the material as flat as possible, and curing at room temperature or medium-low temperature for 2-6 hours;
(4) and a layer of resin curing agent gel is coated on the filling material, so that the binding force between the filled material and the material to be filled is increased. Repeating the steps (1) to (3) when the glue is not completely cured until the mould is filled;
(5) in the last filling procedure, the filling material is higher than the mould by about 1mm, and the filling material is machined into a regular size after being solidified; or a female die is added in the last filling procedure to control the shape and the size of the material.
2. The preparation method of the light integrated composite material according to claim 1, characterized in that the raw materials and the mixture ratio are as follows:
3. the preparation method of the lightweight integrated composite material as claimed in claim 1, wherein the curing temperature in the step (3) is controlled to be 0-50 ℃.
4. The method for preparing a lightweight integrated composite material as claimed in claim 2, wherein the epoxy resin is at least one of bisphenol a type epoxy resin, bisphenol F type epoxy resin and unsaturated polyester resin.
5. The method of claim 1, wherein the curing agent is a curing agent for thermosetting resin.
6. The method for preparing a lightweight integrated composite material as claimed in claim 5, wherein the curing agent for thermosetting resin is at least one of polyamide curing agent, T31 curing agent and isophorone diamine.
7. The method for preparing a lightweight integrated composite material as claimed in claim 1, wherein the density of the hollow glass microspheres is 0.125-0.42 g/cm3。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111193591.5A CN113861622A (en) | 2021-10-13 | 2021-10-13 | Preparation of buoyancy material by integral forming process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111193591.5A CN113861622A (en) | 2021-10-13 | 2021-10-13 | Preparation of buoyancy material by integral forming process |
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| Publication Number | Publication Date |
|---|---|
| CN113861622A true CN113861622A (en) | 2021-12-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111193591.5A Pending CN113861622A (en) | 2021-10-13 | 2021-10-13 | Preparation of buoyancy material by integral forming process |
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| CN (1) | CN113861622A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674358A (en) * | 2017-10-23 | 2018-02-09 | 成都航空职业技术学院 | A kind of water soluble core-mould material and preparation method thereof |
| CN110591291A (en) * | 2019-09-27 | 2019-12-20 | 福建师范大学 | Preparation method of coupling agent modified low-water-absorption solid buoyancy material |
| CN110698815A (en) * | 2019-10-10 | 2020-01-17 | 海洋化工研究院有限公司 | High-strength solid buoyancy material and preparation method thereof |
| CN111267327A (en) * | 2020-03-16 | 2020-06-12 | 沈阳飞机工业（集团）有限公司 | Skin stretch forming die and manufacturing method thereof |
-
2021
- 2021-10-13 CN CN202111193591.5A patent/CN113861622A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674358A (en) * | 2017-10-23 | 2018-02-09 | 成都航空职业技术学院 | A kind of water soluble core-mould material and preparation method thereof |
| CN110591291A (en) * | 2019-09-27 | 2019-12-20 | 福建师范大学 | Preparation method of coupling agent modified low-water-absorption solid buoyancy material |
| CN110698815A (en) * | 2019-10-10 | 2020-01-17 | 海洋化工研究院有限公司 | High-strength solid buoyancy material and preparation method thereof |
| CN111267327A (en) * | 2020-03-16 | 2020-06-12 | 沈阳飞机工业（集团）有限公司 | Skin stretch forming die and manufacturing method thereof |
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Application publication date: 20211231 |